#------------------------------------------------------------------------------
#$Date: 2020-05-23 08:16:07 +0300 (Sat, 23 May 2020) $
#$Revision: 252320 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/34/2243406.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2243406
loop_
_publ_author_name
'Khosa, Muhammad Kaleem'
'Wood, Paul T.'
'Humphrey, Simon M.'
'Harrison, William T. A.'
_publ_section_title
;
Hydrothermal synthesis and crystal structure of
poly[bis(\m~3~-3,4-diaminobenzoato)manganese], a layered coordination
polymer
;
_journal_coeditor_code IS5538
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 909
_journal_page_last 913
_journal_paper_doi 10.1107/S2056989020006805
_journal_volume 76
_journal_year 2020
_chemical_formula_iupac '[Mn (C7 H7 N2 O2)2]'
_chemical_formula_moiety 'C14 H14 Mn N4 O4'
_chemical_formula_sum 'C14 H14 Mn N4 O4'
_chemical_formula_weight 357.23
_chemical_name_systematic
Poly[bis(\m~3~-3,4-diaminobenzoato-\k^3^N^3^,O,O')manganese(II)]
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 104.698(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 11.5171(5)
_cell_length_b 4.4212(2)
_cell_length_c 13.9752(7)
_cell_measurement_reflns_used 5315
_cell_measurement_temperature 180(2)
_cell_measurement_theta_max 26.02
_cell_measurement_theta_min 1.02
_cell_volume 688.32(6)
_computing_cell_refinement
;
HKL Scalepack (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 1998)
;
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor, 1997),
SORTAV (Blessing, 1995)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and ATOMS (Shape Software,
2007)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_method '\w and \f'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0417
_diffrn_reflns_av_unetI/netI 0.0383
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 5
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 5289
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.994
_diffrn_reflns_theta_min 2.053
_exptl_absorpt_coefficient_mu 0.987
_exptl_absorpt_correction_T_max 0.983
_exptl_absorpt_correction_T_min 0.869
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SORTAV; Blessing, 1995)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.724
_exptl_crystal_description slab
_exptl_crystal_F_000 366
_exptl_crystal_size_max 0.230
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_min 0.050
_refine_diff_density_max 0.271
_refine_diff_density_min -0.275
_refine_ls_extinction_coef 0.012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018/3 (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref 1.048
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 119
_refine_ls_number_reflns 1345
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.048
_refine_ls_R_factor_all 0.0423
_refine_ls_R_factor_gt 0.0310
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.5090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0697
_refine_ls_wR_factor_ref 0.0742
_reflns_number_gt 1105
_reflns_number_total 1345
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file is5538sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2243406
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.805
_shelx_estimated_absorpt_t_max 0.952
_shelx_hkl_file
;
-14 0 3 -0.11 2.79
-14 0 4 27.93 3.98
-14 0 5 2.15 3.44
-14 0 6 46.99 5.15
-14 0 7 6.64 4.18
-13 0 1 29.27 3.11
-13 0 2 -3.12 1.72
-13 0 3 61.09 6.69
-13 0 4 0.43 3.23
-13 0 5 217.82 15.55
-13 0 6 5.70 3.98
-13 0 7 46.66 5.05
-13 0 8 8.88 4.39
-13 0 9 188.30 14.33
-13 0 10 -0.32 4.68
13 1 -1 2.53 2.32
13 -1 -1 -0.33 2.60
13 1 -2 50.33 4.24
13 -1 -2 34.48 4.67
13 -1 -3 -0.32 3.25
13 1 -3 -0.74 1.91
13 -1 -4 61.98 5.31
13 1 -4 55.91 6.08
13 1 -5 -2.45 2.35
13 -1 -5 -3.12 2.80
13 1 -6 47.35 5.23
13 -1 -6 52.95 5.38
13 -1 -7 128.30 13.20
13 1 -7 114.58 11.52
13 1 -8 -3.09 3.83
13 -1 -8 6.94 4.49
13 -1 -9 79.98 6.73
13 1 -9 68.24 6.92
13 2 -2 -1.36 2.73
-13 2 2 -6.23 4.81
13 -2 -2 4.69 3.51
13 -2 -3 18.27 4.04
13 2 -3 18.32 3.58
-13 2 3 11.83 3.61
-13 2 4 19.76 3.73
13 2 -4 14.99 3.80
13 -2 -4 10.60 3.92
13 -2 -5 8.15 4.02
-13 2 5 1.98 3.19
13 2 -5 1.38 2.64
13 2 -6 -0.21 3.81
-13 2 6 -0.66 4.41
13 -2 -6 3.38 2.96
-12 0 1 -1.18 2.26
-12 0 2 11.12 2.70
12 0 -2 8.74 2.70
-12 0 3 -3.14 2.13
-12 0 4 57.99 4.55
-12 0 6 262.74 13.52
-12 0 7 -4.62 2.79
-12 0 8 347.67 21.27
-12 0 9 0.85 4.27
-12 0 10 80.28 9.59
-12 0 11 9.66 3.50
-12 0 12 16.42 5.08
12 -1 -1 125.77 8.98
-12 -1 1 122.37 7.47
12 1 -1 117.49 7.84
12 1 -2 31.10 3.19
12 -1 -2 28.26 3.81
12 -1 -2 35.99 4.29
12 -1 -3 27.75 3.01
12 -1 -3 31.12 4.13
12 1 -3 22.89 2.66
12 1 -4 15.36 2.56
12 -1 -4 7.57 3.79
12 -1 -4 17.47 3.22
12 1 -5 108.75 8.13
12 -1 -5 118.94 7.80
12 -1 -5 102.60 8.62
12 1 -6 3.84 3.52
12 -1 -6 0.64 2.68
12 -1 -6 -2.04 3.76
12 1 -7 11.30 2.88
12 -1 -7 20.80 3.33
12 1 -8 2.45 2.88
12 -1 -8 0.11 2.89
12 -1 -9 112.93 10.90
12 1 -9 102.39 8.52
12 -1 -10 -2.13 3.30
12 1 -10 3.61 3.08
12 1 -11 20.87 3.81
12 -1 -11 19.74 3.93
12 -1 -12 10.59 5.19
12 1 -12 8.99 3.70
12 -2 -1 24.92 3.31
12 2 -1 32.87 4.09
-12 2 1 33.63 4.14
12 2 -2 142.44 9.89
12 -2 -2 131.58 11.32
-12 2 2 142.72 10.50
-12 2 3 3.83 4.38
12 -2 -3 -2.33 2.55
12 2 -3 1.90 2.11
-12 2 4 58.45 6.15
12 2 -4 47.34 5.50
12 -2 -4 45.77 5.20
12 2 -5 56.54 6.25
-12 2 5 42.64 6.05
12 2 -6 81.20 9.13
-12 2 6 105.83 8.83
12 -2 -6 83.94 7.00
12 -2 -7 15.11 4.75
12 2 -7 15.70 3.29
12 2 -8 10.92 4.24
12 -2 -8 5.49 3.27
12 2 -9 16.64 3.50
12 -2 -9 15.09 3.69
12 2 -10 4.98 3.28
12 -2 -10 14.97 5.17
11 0 -1 47.85 4.00
-11 0 1 39.98 3.26
-11 0 2 2.13 2.47
11 0 -2 9.09 2.92
-11 0 3 1.90 2.69
11 0 -3 0.11 2.06
11 0 -3 5.94 2.59
11 0 -4 9.52 3.35
11 0 -4 -1.95 1.51
-11 0 4 1.34 2.12
11 0 -5 1447.52 65.97
11 0 -5 1368.41 67.51
11 0 -6 2.69 2.58
11 0 -6 -1.19 2.05
11 0 -7 5.05 3.01
11 0 -7 -0.54 1.73
-11 0 8 -2.78 4.18
-11 0 9 23.07 4.70
-11 0 10 0.43 3.09
-11 0 11 2.44 4.57
-11 0 12 -3.50 3.18
-11 0 13 87.72 8.16
-11 1 1 7.69 2.53
11 -1 -1 1.82 3.21
11 -1 -1 4.04 1.75
-11 -1 1 9.43 2.50
11 1 -1 3.81 2.22
-11 -1 1 4.87 2.21
11 -1 -2 68.21 5.68
-11 -1 2 67.88 4.55
-11 1 2 62.49 4.87
11 1 -2 80.34 5.54
-11 -1 3 0.23 2.03
11 -1 -3 4.12 2.82
11 1 -3 -1.70 2.02
11 -1 -3 0.43 2.04
-11 1 3 2.44 2.77
11 -1 -4 14.29 2.37
11 -1 -4 21.74 3.57
11 1 -4 18.46 2.56
-11 -1 4 6.51 3.48
11 -1 -5 15.64 2.91
11 1 -5 17.30 3.42
11 -1 -5 11.41 2.91
11 -1 -6 56.97 4.66
11 1 -6 51.45 3.85
11 -1 -6 47.87 4.74
11 -1 -7 69.84 7.63
11 -1 -7 62.93 4.58
11 1 -7 71.87 5.45
11 -1 -8 116.20 12.32
11 -1 -8 121.57 8.11
11 1 -8 106.39 8.43
11 1 -9 4.57 2.87
11 -1 -9 8.32 2.85
11 -1 -9 17.50 4.38
11 -1 -10 143.52 11.95
11 1 -10 128.11 11.17
11 1 -11 20.98 4.88
11 -1 -11 20.72 3.83
11 1 -12 70.78 6.78
11 -1 -12 77.50 8.07
-11 1 13 32.96 7.93
-11 -2 1 229.76 18.85
-11 2 1 327.60 17.87
-11 -2 1 306.28 22.06
11 2 -1 333.58 21.00
11 -2 -1 323.39 14.98
-11 2 2 16.23 3.38
-11 -2 2 17.37 2.67
-11 -2 2 4.58 4.24
11 -2 -2 11.44 3.50
11 2 -2 15.04 2.52
-11 2 3 147.66 9.64
11 -2 -3 144.79 10.01
11 2 -3 142.40 8.67
-11 2 4 5.37 3.50
11 -2 -4 3.17 3.70
11 2 -4 9.83 2.43
-11 2 5 13.06 4.06
11 2 -5 17.59 3.29
11 -2 -5 8.35 2.96
11 2 -6 -2.44 3.61
11 -2 -6 10.99 4.33
11 -2 -6 5.60 3.62
11 -2 -7 17.76 3.86
11 -2 -7 14.27 3.38
11 2 -7 22.18 4.14
11 2 -8 -1.70 2.76
11 -2 -8 0.32 2.96
11 -2 -9 98.75 7.95
11 2 -9 93.12 7.76
11 2 -10 8.58 4.45
11 -2 -10 2.74 5.07
11 2 -11 29.33 5.19
11 -2 -11 21.84 4.12
11 3 -1 13.00 2.50
11 -3 -1 24.17 4.22
-11 3 1 23.26 4.22
11 -3 -2 25.01 3.40
-11 3 2 36.11 4.34
11 3 -2 37.87 3.86
11 3 -3 -0.63 3.35
-11 3 3 1.52 4.57
11 -3 -3 0.31 3.91
11 -3 -4 12.17 3.30
-11 3 4 10.02 3.38
11 3 -4 9.56 2.84
11 -3 -5 2.79 3.10
-11 3 5 5.46 4.37
11 3 -5 4.53 2.84
11 3 -6 37.27 4.12
-11 3 6 39.82 4.06
11 -3 -6 41.73 5.40
11 3 -7 12.27 3.39
-11 3 7 13.59 4.06
11 -3 -7 13.49 4.36
-11 3 8 112.83 9.28
11 -3 -8 117.19 9.72
11 3 -8 125.90 11.15
-10 0 1 -0.67 1.90
10 0 -1 0.22 1.73
10 0 -2 265.01 12.92
-10 0 2 229.66 17.91
10 0 -2 281.21 12.23
-10 0 3 1.34 2.34
10 0 -3 0.11 7.78
10 0 -3 3.68 3.03
10 0 -4 13.52 2.27
-10 0 4 7.78 2.67
10 0 -4 11.36 2.49
10 0 -5 3.03 1.95
-10 0 5 0.55 1.89
10 0 -5 2.59 2.48
10 0 -6 17.18 2.06
10 0 -6 10.55 2.80
10 0 -7 -1.51 1.62
10 0 -7 1.50 2.69
10 0 -8 2.16 1.73
10 0 -8 0.32 4.18
10 0 -9 1.08 1.62
10 0 -9 -3.95 2.99
-10 0 10 19.82 3.62
-10 0 11 -0.32 3.19
-10 0 12 51.99 6.05
-10 0 13 -2.65 3.18
-10 0 14 55.24 7.09
-10 -1 1 241.75 10.53
10 -1 -1 218.50 12.52
-10 1 1 219.30 11.56
-10 -1 1 249.68 18.37
10 -1 -1 208.11 12.11
10 1 -1 224.73 10.74
-10 1 2 48.83 4.30
10 -1 -2 48.16 4.04
-10 -1 2 53.19 3.73
10 1 -2 54.56 3.94
-10 -1 2 46.09 3.55
10 -1 -2 59.93 4.32
10 -1 -3 0.32 2.90
-10 1 3 4.53 2.65
10 -1 -3 -3.79 2.82
-10 -1 3 -6.83 2.80
10 1 -3 -5.76 2.66
10 -1 -4 16.93 3.13
-10 -1 4 17.86 3.24
10 -1 -4 14.49 2.60
-10 1 4 13.73 2.33
10 1 -4 8.75 3.10
-10 -1 5 477.80 34.55
-10 1 5 448.91 31.01
10 -1 -5 492.24 36.35
10 -1 -5 520.43 27.21
10 1 -5 506.94 28.61
10 -1 -6 11.19 3.66
10 -1 -6 12.41 2.29
10 1 -6 13.98 2.67
10 -1 -7 126.61 7.08
10 -1 -7 116.40 7.75
10 1 -7 112.78 8.02
10 -1 -8 2.98 1.99
10 -1 -8 5.24 2.78
10 1 -8 5.86 2.66
10 -1 -9 194.34 12.33
10 1 -9 195.60 11.85
10 -1 -10 -0.43 3.09
10 1 -10 2.44 2.87
10 1 -11 39.22 3.93
10 -1 -11 35.41 4.36
10 1 -12 13.98 4.66
10 -1 -12 9.23 3.40
10 1 -13 44.64 6.03
10 -1 -13 42.28 6.36
10 -1 -14 29.73 5.40
10 1 -14 33.30 5.50
-10 -2 1 0.34 1.94
-10 -2 1 2.56 1.67
-10 2 1 4.99 2.06
10 -2 -1 -1.40 2.59
-10 2 1 2.49 2.82
10 -2 -1 1.48 2.32
10 2 -1 4.40 2.52
-10 2 2 167.48 10.57
10 2 -2 174.05 11.70
10 -2 -2 180.15 10.00
10 -2 -2 170.12 10.41
-10 -2 2 152.11 10.56
-10 -2 2 163.03 12.37
-10 -2 3 50.49 4.24
-10 2 3 62.68 4.70
10 -2 -3 49.79 3.95
-10 -2 3 39.59 4.11
10 2 -3 45.92 4.65
10 -2 -3 48.65 4.02
-10 2 4 169.89 10.10
10 2 -4 155.66 11.35
10 -2 -4 159.85 8.12
10 -2 -4 159.17 9.98
10 -2 -5 9.93 2.85
-10 2 5 11.95 2.85
10 2 -5 11.98 2.54
10 -2 -5 13.00 3.97
10 2 -6 17.51 2.97
10 -2 -6 15.32 3.17
10 -2 -6 24.72 4.22
10 -2 -7 4.35 2.68
10 2 -7 11.04 3.93
10 -2 -7 6.76 4.12
10 -2 -8 112.46 8.38
10 2 -8 131.40 10.96
10 -2 -9 15.54 3.49
10 2 -9 25.57 3.51
10 2 -10 108.15 8.41
10 -2 -10 120.05 10.70
10 -2 -11 13.63 3.70
10 2 -11 15.47 4.77
10 2 -12 55.80 7.53
10 -2 -12 61.13 7.30
10 2 -13 16.72 4.34
10 -2 -13 17.09 4.01
10 3 -1 -1.77 3.02
10 -3 -1 1.13 2.77
-10 3 1 -3.02 4.43
10 -3 -2 0.62 2.78
10 3 -2 0.42 2.30
-10 3 2 4.44 4.33
10 -3 -3 158.48 9.55
-10 3 3 155.11 10.47
10 3 -3 149.91 10.08
10 -3 -4 3.30 2.99
10 3 -4 7.25 2.73
-10 3 4 1.20 7.18
10 3 -5 37.42 4.12
10 -3 -5 31.54 4.66
-10 3 5 46.09 4.16
-10 3 6 13.97 4.26
10 -3 -6 16.38 3.84
10 3 -6 20.50 3.38
10 -3 -7 76.27 7.71
10 3 -7 68.47 6.89
-10 3 7 73.93 5.72
10 -3 -8 -5.94 4.69
-10 3 8 1.64 2.41
10 3 -8 7.63 4.45
10 -3 -9 18.05 5.22
-10 3 9 14.14 2.74
10 3 -9 13.46 3.50
10 3 -10 3.82 3.29
10 -3 -10 0.52 8.57
9 0 -1 182.35 7.49
9 0 -1 193.83 9.38
-9 0 1 166.96 10.06
9 0 -2 2.48 2.38
9 0 -2 -1.63 2.71
-9 0 2 -1.11 2.22
9 0 -3 22.87 2.60
9 0 -3 18.60 2.49
-9 0 3 13.98 2.00
9 0 -4 -2.38 1.95
-9 0 4 2.88 1.77
9 0 -4 1.41 2.70
9 0 -5 259.08 10.17
9 0 -5 270.18 12.28
-9 0 5 213.98 11.45
9 0 -6 0.65 2.58
9 0 -6 -0.86 1.73
-9 0 6 -0.22 1.98
9 0 -7 37.81 2.93
9 0 -7 43.16 4.62
-9 0 7 39.10 3.31
9 0 -8 3.58 1.84
9 0 -8 5.46 4.28
9 0 -9 4.49 1.86
9 0 -9 -3.10 2.99
-9 0 10 4.48 4.37
-9 0 11 61.16 4.80
-9 0 12 -2.76 3.19
-9 0 13 98.46 7.55
-9 0 14 2.23 4.56
-9 0 15 4.03 3.50
-9 -1 1 142.01 6.58
-9 1 1 147.82 7.69
9 1 -1 145.95 7.02
9 -1 -1 140.95 7.79
-9 -1 1 139.00 8.39
9 -1 -1 151.11 6.71
-9 -1 2 277.79 16.38
9 -1 -2 275.54 13.58
-9 -1 2 238.78 15.73
9 -1 -2 284.50 10.78
-9 1 2 290.41 13.04
9 1 -2 286.25 12.39
9 -1 -3 446.68 26.44
-9 1 3 446.06 23.48
-9 -1 3 411.87 21.13
9 1 -3 476.50 20.68
9 -1 -3 445.29 19.45
-9 1 4 341.57 17.55
9 1 -4 330.27 15.76
9 -1 -4 365.90 17.21
9 -1 -4 325.12 23.08
-9 -1 4 306.57 20.76
9 -1 -5 30.38 4.10
9 1 -5 38.94 3.10
9 -1 -5 33.32 2.85
-9 -1 5 31.98 3.33
-9 1 5 36.27 3.88
9 -1 -6 226.59 16.61
9 -1 -6 254.58 12.28
-9 -1 6 211.19 15.63
9 1 -6 236.84 11.06
-9 1 6 202.26 11.68
9 1 -7 7.88 4.16
9 -1 -7 7.72 2.79
9 -1 -8 71.18 5.79
9 1 -8 77.79 5.87
9 1 -9 3.19 3.72
9 -1 -9 -0.32 3.85
9 1 -10 96.08 7.35
9 -1 -10 99.36 8.01
9 1 -11 0.64 2.86
9 -1 -11 6.92 2.98
9 1 -12 66.56 6.48
9 -1 -12 71.50 5.75
9 1 -13 0.11 3.28
9 -1 -13 4.46 3.40
9 -1 -14 29.36 4.67
9 1 -14 39.08 6.46
9 1 -15 16.52 3.81
9 -1 -15 12.82 3.71
9 -2 -1 397.90 18.67
-9 2 1 352.07 18.33
-9 2 1 366.93 22.80
9 2 -1 404.89 16.45
-9 -2 1 346.76 21.23
-9 -2 1 344.09 28.58
9 -2 -1 354.06 20.41
-9 -2 2 0.22 1.88
9 -2 -2 -1.68 2.42
9 -2 -2 3.71 2.73
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-11 1 -3 14.95 3.36
-11 -1 -3 10.27 4.47
-11 1 -4 50.77 5.93
-11 1 -4 48.07 5.51
-11 -1 -4 74.85 6.39
-11 1 -5 -0.66 3.62
-11 1 -5 3.45 3.23
-11 -1 -5 2.80 3.59
-11 1 -6 62.42 6.35
-11 -1 -6 57.41 6.51
-11 -1 -6 57.69 5.21
11 2 0 6.58 2.40
-11 2 0 9.64 4.33
-11 -2 0 3.25 2.91
11 -2 0 0.43 3.08
11 2 1 88.01 5.32
-11 2 -1 91.53 7.03
-11 -2 -1 93.26 8.57
11 -2 1 88.14 6.23
-11 2 -2 -2.70 4.64
-11 -2 -2 -1.47 2.48
11 -2 2 0.11 1.60
-11 2 -3 116.02 7.98
-11 -2 -3 99.44 8.28
-11 2 -4 -2.79 3.22
-11 -2 -4 1.25 4.30
-11 2 -5 42.93 5.15
-11 -2 -5 47.58 5.11
11 3 0 18.16 3.11
-11 3 0 12.85 5.08
11 -3 0 11.01 3.81
-11 3 -1 -2.91 4.96
11 -3 1 4.74 3.40
12 0 0 62.17 5.58
12 0 1 1.17 1.60
-12 0 -1 -5.07 2.98
12 0 2 142.06 10.54
-12 0 -3 8.62 5.42
-12 0 -3 -0.55 3.07
-12 0 -4 43.64 6.10
-12 0 -4 55.56 5.69
-12 0 -5 5.99 3.99
-12 0 -5 -2.17 3.15
12 1 0 16.85 2.32
-12 1 0 18.11 3.62
-12 -1 0 12.99 4.00
12 -1 0 14.93 2.18
-12 1 -1 42.64 6.02
-12 -1 -1 48.06 4.24
12 -1 1 48.90 5.24
-12 1 -2 3.05 3.27
-12 -1 -2 -7.47 4.24
-12 1 -3 68.53 6.85
-12 -1 -3 76.16 6.73
-12 1 -4 -7.80 4.77
-12 -1 -4 -0.56 4.93
12 2 0 37.89 4.07
-12 2 0 47.33 4.56
12 -2 0 36.31 4.29
-12 2 -1 -2.17 4.87
12 -2 1 -3.86 2.68
-12 2 -2 10.37 5.19
-12 -2 -2 -1.13 3.73
-13 1 0 48.26 4.95
-13 -1 0 50.96 5.46
-13 1 -1 12.27 3.73
-13 -1 -1 -0.45 3.12
-13 -1 -1 -0.45 3.12
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 34362
_shelx_res_file
;
TITL pw0710 in P2(1)/n
pw0710t.res
created by SHELXL-2018/3 at 18:27:25 on 19-Mar-2020
CELL 0.71073 11.5171 4.4212 13.9752 90 104.698 90
ZERR 2 0.0005 0.0002 0.0007 0 0.003 0
LATT 1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H N O MN
UNIT 28 28 8 8 2
L.S. 4
BOND $H
conf
FMAP 2
PLAN 10
ACTA
htab
eqiv $1 x,y-1,z
mpla 3 c7 o1 o2 mn1 mn1_$1
mpla 6 c1 c2 c3 c4 c5 c6 n1 n2 c7
TEMP -93
SIZE 0.23 0.1 0.05
rem yellow(?) slab
REM Instructions for potential hydrogen bonds
EQIV $3 -x+1/2, y+1/2, -z+1/2
HTAB N1 O1_$3
EQIV $8 -x+3/2, y-1/2, -z+1/2
HTAB N2 N2_$8
EQIV $9 x+1/2, -y-1/2, z+1/2
HTAB N2 O2_$9
WGHT 0.028200 0.509000
EXTI 0.011512
FVAR 0.59725
MN1 5 0.000000 0.500000 0.000000 10.50000 0.01897 0.01729 =
0.01865 0.00021 0.00188 0.00075
C1 1 0.321859 -0.048844 0.117171 11.00000 0.01942 0.01878 =
0.01961 0.00233 0.00343 -0.00101
C2 1 0.364142 0.105477 0.205980 11.00000 0.01979 0.01765 =
0.02245 0.00213 0.00640 0.00215
AFIX 43
H2 2 0.312438 0.241153 0.228031 11.00000 -1.20000
AFIX 0
C3 1 0.480369 0.064241 0.262641 11.00000 0.01976 0.02002 =
0.01710 0.00132 0.00329 -0.00275
C4 1 0.557986 -0.133482 0.230631 11.00000 0.01652 0.02030 =
0.02380 0.00387 0.00406 -0.00147
C5 1 0.516339 -0.280230 0.139849 11.00000 0.02326 0.02761 =
0.02653 -0.00220 0.00878 0.00595
AFIX 43
H5 2 0.568982 -0.407707 0.115733 11.00000 -1.20000
AFIX 0
C6 1 0.399253 -0.241873 0.084702 11.00000 0.02579 0.02564 =
0.02008 -0.00283 0.00360 0.00091
AFIX 43
H6 2 0.371484 -0.348284 0.024144 11.00000 -1.20000
AFIX 0
C7 1 0.194018 -0.012238 0.060789 11.00000 0.01982 0.01759 =
0.01678 0.00424 0.00440 -0.00304
N1 3 0.521605 0.216931 0.355412 11.00000 0.01887 0.01821 =
0.02298 -0.00207 0.00275 -0.00175
H1N 2 0.482165 0.386904 0.358527 11.00000 -1.20000
H2N 2 0.595986 0.262389 0.364573 11.00000 -1.20000
N2 3 0.677631 -0.166334 0.287470 11.00000 0.01855 0.02732 =
0.02320 0.00129 0.00582 0.00374
H3N 2 0.715721 -0.305943 0.266862 11.00000 -1.20000
H4N 2 0.680561 -0.189505 0.350414 11.00000 -1.20000
O1 4 0.133703 0.197540 0.085857 11.00000 0.02080 0.02149 =
0.02343 0.00130 0.00261 0.00472
O2 4 0.150109 -0.199783 -0.008406 11.00000 0.02275 0.02316 =
0.02152 -0.00168 0.00309 -0.00225
HKLF 4
REM pw0710 in P2(1)/n
REM wR2 = 0.0742, GooF = S = 1.048, Restrained GooF = 1.048 for all data
REM R1 = 0.0310 for 1105 Fo > 4sig(Fo) and 0.0423 for all 1345 data
REM 119 parameters refined using 0 restraints
END
WGHT 0.0282 0.5088
REM Instructions for potential hydrogen bonds
HTAB N1 O1_$3
HTAB N2 N2_$8
HTAB N2 O2_$9
REM Highest difference peak 0.271, deepest hole -0.275, 1-sigma level 0.061
Q1 1 0.5057 -0.0822 0.2564 11.00000 0.05 0.27
Q2 1 0.4140 0.0341 0.2469 11.00000 0.05 0.25
Q3 1 0.2702 0.0112 0.0868 11.00000 0.05 0.25
Q4 1 0.5043 0.1309 0.2935 11.00000 0.05 0.24
Q5 1 0.4677 0.0890 0.3927 11.00000 0.05 0.20
Q6 1 0.7017 -0.0131 0.2548 11.00000 0.05 0.20
Q7 1 0.7145 -0.0493 0.4002 11.00000 0.05 0.19
Q8 1 0.5853 -0.3074 0.0993 11.00000 0.05 0.19
Q9 1 0.4389 0.1454 0.2281 11.00000 0.05 0.18
Q10 1 0.5319 0.0532 0.3812 11.00000 0.05 0.18
;
_shelx_res_checksum 6511
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn1 0.000000 0.500000 0.000000 0.01883(17) Uani d 1 . .
C C1 0.32186(18) -0.0488(5) 0.11717(15) 0.0195(5) Uani d 1 . .
C C2 0.36414(18) 0.1055(5) 0.20598(15) 0.0198(5) Uani d 1 . .
H H2 0.312438 0.241153 0.228031 0.024 Uiso calc 1 . .
C C3 0.48037(18) 0.0642(5) 0.26264(15) 0.0192(5) Uani d 1 . .
C C4 0.55799(18) -0.1335(5) 0.23063(16) 0.0204(5) Uani d 1 . .
C C5 0.51634(19) -0.2802(5) 0.13985(17) 0.0254(5) Uani d 1 . .
H H5 0.568982 -0.407707 0.115733 0.030 Uiso calc 1 . .
C C6 0.39925(19) -0.2419(5) 0.08470(16) 0.0242(5) Uani d 1 . .
H H6 0.371484 -0.348284 0.024144 0.029 Uiso calc 1 . .
C C7 0.19402(18) -0.0122(5) 0.06079(14) 0.0181(4) Uani d 1 . .
N N1 0.52161(17) 0.2169(4) 0.35541(13) 0.0205(4) Uani d 1 . .
H H1N 0.482(2) 0.387(6) 0.3585(18) 0.025 Uiso d 1 . .
H H2N 0.596(2) 0.262(6) 0.3646(18) 0.025 Uiso d 1 . .
N N2 0.67763(16) -0.1663(5) 0.28747(15) 0.0229(4) Uani d 1 . .
H H3N 0.716(2) -0.306(6) 0.2669(18) 0.028 Uiso d 1 . .
H H4N 0.681(2) -0.190(6) 0.350(2) 0.028 Uiso d 1 . .
O O1 0.13370(12) 0.1975(3) 0.08586(11) 0.0224(4) Uani d 1 . .
O O2 0.15011(13) -0.1998(3) -0.00841(11) 0.0229(4) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Mn1 0.0190(3) 0.0173(3) 0.0187(3) 0.00075(19) 0.00188(18) 0.00021(19)
C1 0.0194(10) 0.0188(12) 0.0196(10) -0.0010(8) 0.0034(9) 0.0023(8)
C2 0.0198(10) 0.0176(11) 0.0225(11) 0.0022(8) 0.0064(9) 0.0021(9)
C3 0.0198(10) 0.0200(12) 0.0171(10) -0.0027(8) 0.0033(8) 0.0013(8)
C4 0.0165(10) 0.0203(11) 0.0238(11) -0.0015(9) 0.0041(9) 0.0039(9)
C5 0.0233(11) 0.0276(13) 0.0265(12) 0.0059(10) 0.0088(9) -0.0022(10)
C6 0.0258(11) 0.0256(12) 0.0201(11) 0.0009(10) 0.0036(9) -0.0028(9)
C7 0.0198(10) 0.0176(10) 0.0168(10) -0.0030(9) 0.0044(8) 0.0042(9)
N1 0.0189(9) 0.0182(10) 0.0230(9) -0.0018(8) 0.0027(8) -0.0021(8)
N2 0.0185(9) 0.0273(11) 0.0232(10) 0.0037(8) 0.0058(8) 0.0013(9)
O1 0.0208(8) 0.0215(8) 0.0234(8) 0.0047(6) 0.0026(6) 0.0013(6)
O2 0.0227(8) 0.0232(8) 0.0215(8) -0.0022(6) 0.0031(6) -0.0017(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Mn1 O1 . 3_565 180.0 ?
O1 Mn1 O2 . 3 93.20(6) ?
O1 Mn1 O2 3_565 3 86.80(6) ?
O1 Mn1 O2 . 1_565 86.80(6) ?
O1 Mn1 O2 3_565 1_565 93.20(6) ?
O2 Mn1 O2 3 1_565 180.0 ?
O1 Mn1 N1 . 4_565 90.52(6) ?
O1 Mn1 N1 3_565 4_565 89.48(6) ?
O2 Mn1 N1 3 4_565 93.25(6) ?
O2 Mn1 N1 1_565 4_565 86.75(6) ?
O1 Mn1 N1 . 2 89.48(6) ?
O1 Mn1 N1 3_565 2 90.52(6) ?
O2 Mn1 N1 3 2 86.75(6) ?
O2 Mn1 N1 1_565 2 93.25(6) ?
N1 Mn1 N1 4_565 2 180.0 ?
C6 C1 C2 . . 118.93(19) ?
C6 C1 C7 . . 121.50(18) ?
C2 C1 C7 . . 119.54(19) ?
C3 C2 C1 . . 121.0(2) ?
C3 C2 H2 . . 119.5 ?
C1 C2 H2 . . 119.5 ?
C2 C3 C4 . . 120.14(19) ?
C2 C3 N1 . . 120.44(19) ?
C4 C3 N1 . . 119.41(18) ?
C5 C4 C3 . . 118.65(19) ?
C5 C4 N2 . . 121.6(2) ?
C3 C4 N2 . . 119.64(19) ?
C6 C5 C4 . . 120.7(2) ?
C6 C5 H5 . . 119.7 ?
C4 C5 H5 . . 119.7 ?
C5 C6 C1 . . 120.6(2) ?
C5 C6 H6 . . 119.7 ?
C1 C6 H6 . . 119.7 ?
O1 C7 O2 . . 123.23(18) ?
O1 C7 C1 . . 118.20(18) ?
O2 C7 C1 . . 118.53(19) ?
C3 N1 Mn1 . 2_545 120.83(14) ?
C3 N1 H1N . . 112.9(16) ?
Mn1 N1 H1N 2_545 . 98.0(16) ?
C3 N1 H2N . . 109.6(17) ?
Mn1 N1 H2N 2_545 . 107.0(17) ?
H1N N1 H2N . . 107(2) ?
C4 N2 H3N . . 113.5(17) ?
C4 N2 H4N . . 111.1(16) ?
H3N N2 H4N . . 111(2) ?
C7 O1 Mn1 . . 131.83(13) ?
C7 O2 Mn1 . 1_545 121.03(13) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O1 . 2.1591(14) ?
Mn1 O1 3_565 2.1591(14) ?
Mn1 O2 3 2.2062(15) ?
Mn1 O2 1_565 2.2062(15) ?
Mn1 N1 4_565 2.3065(19) ?
Mn1 N1 2 2.3065(19) ?
C1 C6 . 1.391(3) ?
C1 C2 . 1.392(3) ?
C1 C7 . 1.492(3) ?
C2 C3 . 1.384(3) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.402(3) ?
C3 N1 . 1.432(3) ?
C4 C5 . 1.397(3) ?
C4 N2 . 1.413(3) ?
C5 C6 . 1.383(3) ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
C7 O1 . 1.261(3) ?
C7 O2 . 1.277(3) ?
N1 H1N . 0.88(3) ?
N1 H2N . 0.86(3) ?
N2 H3N . 0.85(3) ?
N2 H4N . 0.88(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1N O1 2 0.88(3) 2.19(3) 3.022(3) 156(2) yes
N2 H3N N2 2_645 0.85(3) 2.26(3) 3.106(3) 178(2) yes
N2 H4N O2 4_656 0.88(3) 2.15(3) 3.008(2) 167(2) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . -1.4(3) ?
C7 C1 C2 C3 . . . . 176.57(19) ?
C1 C2 C3 C4 . . . . 0.5(3) ?
C1 C2 C3 N1 . . . . -178.0(2) ?
C2 C3 C4 C5 . . . . 1.6(3) ?
N1 C3 C4 C5 . . . . -179.9(2) ?
C2 C3 C4 N2 . . . . 177.9(2) ?
N1 C3 C4 N2 . . . . -3.5(3) ?
C3 C4 C5 C6 . . . . -2.9(3) ?
N2 C4 C5 C6 . . . . -179.1(2) ?
C4 C5 C6 C1 . . . . 2.0(3) ?
C2 C1 C6 C5 . . . . 0.1(3) ?
C7 C1 C6 C5 . . . . -177.8(2) ?
C6 C1 C7 O1 . . . . -169.7(2) ?
C2 C1 C7 O1 . . . . 12.4(3) ?
C6 C1 C7 O2 . . . . 12.3(3) ?
C2 C1 C7 O2 . . . . -165.55(19) ?
C2 C3 N1 Mn1 . . . 2_545 89.4(2) ?
C4 C3 N1 Mn1 . . . 2_545 -89.1(2) ?
O2 C7 O1 Mn1 . . . . -40.5(3) ?
C1 C7 O1 Mn1 . . . . 141.59(15) ?
O1 C7 O2 Mn1 . . . 1_545 -60.8(2) ?
C1 C7 O2 Mn1 . . . 1_545 117.02(17) ?
_cod_database_fobs_code 2243406